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Issue 5, 2016
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Synthesis and structural characterization of Zn-containing DAF-1

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Abstract

A study exploring the use of ionic liquid reactions based on imidazolium halides in molecular sieve synthesis has produced a novel zincoaluminophosphate material with an open DFO-type framework structure. This framework structure had only been observed previously in the magnesioaluminophosphate system (Mg-DAF-1) where decamethonium was used as the structure directing agent. The new Zn-DAF-1 material has been characterized using chemical and thermogravimetric analysis and 13C, 19F, 27Al and 31P MAS NMR techniques. Structure analysis (P6/mcc, a = 22.2244(1) Å, c = 42.3293(3) Å) using synchrotron powder diffraction data not only confirmed the framework structure, but also revealed the locations of the Al, P and Zn atoms in the framework, the N,N′-di-isopropyl-imidazolium (DIPI) ions in the pores, some fluoride ions associated with double 4-rings, and some water molecules and anions filling the remaining space. This level of structural detail had not been possible in the Mg-DAF-1 material. Four different locations for the DIPI cation were found in the two 12-ring channels and Zn was found to substitute for only one of the six crystallographically distinct Al sites to yield the approximate crystal chemical formula |(DIPI)17(OH,F)11(H2O)23|[Zn6Al126P132O528]-DFO.

Graphical abstract: Synthesis and structural characterization of Zn-containing DAF-1

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Supplementary files

Article information


Submitted
19 Oct 2015
Accepted
27 Nov 2015
First published
02 Dec 2015

New J. Chem., 2016,40, 4160-4166
Article type
Paper
Author version available

Synthesis and structural characterization of Zn-containing DAF-1

A. B. Pinar, L. B. McCusker, C. Baerlocher, S. Hwang, D. Xie, A. I. Benin and S. I. Zones, New J. Chem., 2016, 40, 4160
DOI: 10.1039/C5NJ02897C

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